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Chenweravanich 2022 - Bond Durability of A Repaired Resin Composite Using A Universal Adhesive and Different Surface Treatments
Chenweravanich 2022 - Bond Durability of A Repaired Resin Composite Using A Universal Adhesive and Different Surface Treatments
Chenweravanich 2022 - Bond Durability of A Repaired Resin Composite Using A Universal Adhesive and Different Surface Treatments
RESEARCH
Purpose: To evaluate the long-term effect of different surface treatments on the repair microtensile bond strength
(μTBS) of resin composite using a universal adhesive.
Materials and Methods: Thirty-six resin composite blocks were fabricated and aged in 37°C distilled water for
1 month. The blocks were randomly assigned to different surface treatments: no treatment (control); diamond bur
grinding (D); diamond bur + phosphoric acid cleaning (DP); diamond bur + silane application (DSi); diamond bur +
phosphoric acid + silane (DPSi); and grit blasting with 50 μm Al2O3 particles + phosphoric acid + silane (APSi).
Thereafter, Single Bond Universal adhesive was applied and repaired with the same composite. Composite-com-
posite stick-shaped specimens were fabricated and subjected to the μTBS test either after 37°C water storage for
24 h or thermocycling for 10,000 cycles. Roughness of different surface-prepared specimens was measured by
profilometer. Data were analysed using ANOVA and Duncan’s post-hoc test (α = 0.05). Failure mode and micromor-
phology of different surface-prepared specimens were observed with SEM and EDS analysis.
Results: The highest μTBS was found in DPSi group at 24 h, and was significantly higher than others. The bond
strengths in all thermocycled groups were significantly lower than those measured at 24 h. The highest μTBS was
also found in the DPSi group, but this did not significantly differ from the DSi group.
Conclusion: Thermocycling significantly reduced the repair bond strength. Diamond bur roughening with application
of silane and universal adhesive yielded the highest repair bond strength for the aged resin composite.
Keywords: bond durability, resin composite repair, surface treatments, universal adhesive.
J Adhes Dent 2022; 24: 67–76. Submitted for publication: 10.06.21; accepted for publication: 23.08.21
doi: 10.3290/j.jad.b2288293
Table 1 Composition and instructions for use of materials used in the study
cedures relies on several factors, such as the surface MATERIALS AND METHODS
characteristics, wettability of the chemical bonding agents,
and chemical composition of the composites.15,21,23 The restorative materials used in the present study, along
Surface roughness is crucial for composite repair and with their classification, manufacturers, batch numbers,
can be achieved mechanically using several techniques, eg, compositions, and directions for use, are presented in
grit blasting with aluminum oxide particles,2,4,6,7,15,36 etch- Table 1. A total of 36 resin composite blocks were built
ing with hydrofluoric acid,4,14,15 and roughening with dia- using the A1 body shade of a nanofilled resin-based com-
mond burs.2,6,7,15,24 In addition to micromechanical reten- posite (Filtek Z350XT, 3M Oral Care; St Paul, MN, USA).
tion, chemical bonding is also a desirable method to The specimens were fabricated using a silicone mold with
increase the bond strength of repaired composite.4 Silane dimensions of 4 mm x 8 mm x 4 mm. The composite was
coupling agents chemically bond the fillers of the old resin placed into the mold in two 2-mm increments. Each incre-
composite to the organic resin matrix of the new one.16,17 ment was light cured for 20 s using an LED light-curing unit
Therefore, the application of a silane coupling agent is rec- (Bluephase, Ivoclar Vivadent; Schaan, Liechtenstein) with a
ommended for resin composite repair.31 light intensity of 1200 mW/cm2 as measured by a radiom-
Dental adhesives also play an important role in the re- eter (Bluephase meter; Ivoclar Vivadent). Prior to photopoly-
pair-composite bond strength by increasing the wettability merizing the second increment, a glass microscope slide
of the pre-treated, silanized surface.5 Recently, a new gen- was used to cover and compress the composite to obtain a
eration of adhesives called “multi-mode” or “universal” ad- flat surface. After that, the resin composite blocks were
hesives has been introduced. Most of them contain acidic removed from the mold. Each block was additionally cured
functional monomer, 10-methacryloyloxydecyl dihydrogen from the top surface for 20 s. The top surface (4 x 8 mm2)
phosphate (10-MDP), and silane. Consequently, this would was then polished with 600-grit SiC abrasive paper under
enable bonding to various substrates without the need for water cooling for 15 s,15 to obtain a homogenous surface.
a separate primer, ie, a silane coupling agent. Considering Subsequently, the blocks were ultrasonically cleaned for
that cavity surfaces for composite repair may include vari- 5 min and stored in distilled water at 37°C for 30 days in
ous substrates, eg, dentin, enamel, and composite, a uni- an incubator to simulate the aging process.9 Aged speci-
versal adhesive may be more user friendly and less time mens were randomly allocated to 6 experimental groups
consuming for repair procedures. (n = 6) according to the repair bonding procedures.
At present, there is limited information on different repair Six blocks of each group were subjected to one of 6 differ-
systems with various conditioning protocols using the uni- ent surface treatments: group C (control): no further treat-
versal adhesive. Therefore, the aim of this study was to ment was performed on the composite surface; group D:
evaluate the long-term effects of different surface treat- roughening with an extra-fine diamond bur (#837 KREF 314
ments on the repair bond strength of resin composite using 014, ISO 806 314 158 504 014, Komet; Lemgo, Germany)
a universal adhesive. The tested null hypotheses are that mounted in a high-speed handpiece at 200,000 rpm, parallel
surface treatments and artificial aging by thermocycling do to the surface, then cleaned with air-water spray for 30 s,
not have an effect on the repair bond strength. and air dried for 10 s; group DP: roughening with diamond
1 mm
New
composite
Surface
treatments
8 mm
4 mm
4 mm
Aged composite
4 mm
8 mm
Fig 1 Schematic procedure of the specimen preparation and microtensile bond strength test set-up.
bur as previously described, plus phosphoric acid cleaning; blade under water cooling in a sectioning machine (IsoMet
group DSi: roughening with diamond bur and silane applica- 1000, Buehler; Lake Bluff, IL, USA). Ten central specimens
tion; group DPSi: roughening with diamond bur, phosphoric were obtained from each block, with a bonding area of ap-
acid cleaning, then silane application; group APSi: the sur- proximately 1 x 1 mm2 (Fig 1). Five stick specimens were
face was grit-blasted with 50-μm aluminum oxide powder for randomly selected for 24-h storage in distilled water at
10 s at a working distance of 10 mm under a pressure of 37°C. The remaining five specimens were allocated to ther-
40 psi using an intra-oral grit blaster (KCP-1000 Whisper Jet, mocycling (5°C-55°C, dwell time 30 s, transfer time 4 s)22
American Dental Airsonic Technologies; Corpus Christi, TX, for 10,000 cycles (TC 301, Medical and Environmental
USA), then cleaned with air-water spray for 30 s, air dried for Equipment Research Laboratory; Bangkok, Thailand).
10 s, cleaned with phosphoric acid, followed by silane appli-
cation. The uses of phosphoric acid gel and silane coupling Microtensile Bond Strength(μTBS) Test
agent strictly followed the instructions as noted in Table 1. The cross-sectional area of each specimen was measured
After the surface treatments, Single Bond Universal Ad- by a digital caliper (Mitutoyo; Tokyo, Japan). Then, each
hesive (3M Oral Care) was applied to the specimens using bonded stick was attached to a jig in a universal testing
a rubbing action for 20 s. Specimens were then gently air machine (LF plus, Lloyd Instruments; Bognor Regis, UK)
blown for 5 s to evaporate the solvent and spread the adhe- using a cyanoacrylate adhesive (Model Repair II Blue,
sive into a thin film. This was then light cured for 10 s ac- Dentsply-Sankin; Otawara, Japan). Each specimen was
cording to the manufacturer’s instructions. loaded in tension until fracture at a crosshead speed of
1 mm/min. The force at failure was utilized to calculate the
Repair Procedures microtensile bond strength using the following equation:
A silicone mold of 4 mm x 8 mm x 8 mm was used. After m = F/A, where m = μTBS (MPa), F = load at failure (N), and
the respective surface treatments and bonding procedures, A = area at the bonded interface (mm2). The mean bond
each specimen was inserted into the mold, leaving a 4-mm strength obtained from each block was used for data
space to be filled by the fresh composite. Care was taken analysis. Pre-test failures, if any, were recorded as 0 MPa
not to contaminate the prepared surface. The A4 body and were included in the calculation.
shade of the nanofilled resin-based composite (Filtek
Z350XT; 3M Oral Care) was incrementally inserted and light Failure Mode Analysis
cured in the same manner as described above. All speci- After the microtensile bond strength test, the fractured
mens were removed from the mold, and then stored in dis- specimens were positioned on an aluminum stub with a
tilled water for 24 h at 37°C in the incubator prior to micro- carbon double-sided tape, then coated with a palladium
tensile bond strength testing. conductive layer via sputtering (SC7620 Mini Sputter
Coater; Quorum Technologies; Lewes, UK). The specimens
Specimen Preparation for Bond Strength Testing were examined with SEM (JSM-6610LV, JEOL; Tokyo,
The repaired composite blocks were sectioned perpendicu- Japan) at 80X magnification. Failure modes were classified
lar to the bonding interface using a slow-speed diamond as follows:20
a
b
b b MPa of the resin composite
60 with different repair proto-
c c
c cols after 24 h and 10,000
50
cycles of thermocycling.
d d
40 e
Mean values with the same
e superscript letters are not
30 f statistically different (two-
way ANOVA and Duncan’s
20 multiple comparison test,
p > 0.05).
10
0
C D DP DSi DPSi APSi
24 h 10,000 TC
100%
Fig 3 Failure analysis of
the specimens using differ-
90% ent surface treatments,
80% and with or without artificial
aging. TC: thermocycling.
70%
60%
50%
40%
30%
20%
10%
0%
Control 24 h Control TC D 24 h D TC DP 24 h DP TC DSi 24 h DSi TC DPSi 24 h DPSi TC APSi 24 h APSi TC
y Type I: adhesive failure – fractured area involved at least Micromorphological Observation and Energy
75% of the interface between resin composite and ad- Dispersive X-ray Spectroscopy of Prepared Surfaces
hesive. Eighteen slices (4 mm x 6 mm x 2 mm) of the nanofilled
y Type II: cohesive failure – fractured area involved at least resin-based composite (Filtek Z350XT; 3M Oral Care) were
75% within the resin composite or adhesive. examined for each group (n = 3). The specimens were pre-
y Type III: mixed failure – fractured area involved both ad- pared and surfaces polished with 600-grit SiC abrasive
hesive failure and cohesive failure in resin composite or paper under running water for 15 s, and then ultrasonically
adhesive, each less than 75%. cleaned in distilled water for 5 min. The slices were as-
c d
e f
signed to 6 different surface treatments: 1. the control; 2. face treatments (n = 5): 1. control; 2. diamond bur roughen-
diamond bur roughening with and 3. without phosphoric ing with and 3. without phosphoric acid cleaning; 4. Grit
acid cleaning; 4. grit blasting with and 5. without phos- blasting with phosphoric acid cleaning; 5. grit blasting with
phoric acid cleaning; and 6. grit blasting with ultrasonic ultrasonic cleaning. Surface roughness (Ra in μm) was mea-
cleaning. After that, the specimens were coated with palla- sured on each specimen using a surface profilometer (Taly-
dium, and the surface morphology was observed using SEM surf Series 2, Taylor Hobson; Leicester, UK) with five succes-
at 1000X, 2000X, and 3000X magnifications. sive measurements in different directions for all specimens.
Energy dispersive x-ray spectroscopy (EDS X-Max; Oxford The mean value was calculated for each subgroup.
Instruments; Bristol, UK) was used to determine the elemen-
tal compositions of the prepared composite surfaces. The Statistical Analysis
amounts of C, O, Si, and Al were measured at 500X magnifi- The microtensile bond strength and surface roughness data
cation. Data were obtained using an SEM (JSM-6610LV; were analyzed for normal distribution using the Kolmogorov-
JEOL) with an attached EDS x-ray detector. Smirnov test. Two-way ANOVA was performed on the micro-
tensile bond strengths, while one-way ANOVA was calculated
Surface Roughness Measurement for the surface roughness. Duncan’s test was performed to
Additional 25 slices (4 mm x 3 mm x 2 mm) of the nanofilled detect statistical differences between the variables and
resin-based composite (Filtek Z350XT; 3M Oral Care) were compare the groups. All tests were performed at a 5% sig-
prepared and divided into five subgroups according to sur- nificance level using SPSS v 20.0 (IBM; Armonk, NY, USA).
a b c d e f
Fig 6 SEM images (top) and EDS mapping of the elemental distributions on the prepared composite surfaces. a. Grinding with 600-grit SiC
paper; b. diamond bur roughening; c. diamond bur roughening followed by phosphoric acid cleaning; d. grit blasting; e. grit blasting followed by
phosphoric acid cleaning; f. grit blasting followed by ultrasonic cleaning. C: carbon; O: oxygen; Si: silicon; Al: aluminum.
ment of fillers, can be observed on the composite substrate grit-blasted and phosphoric-acid cleaned, and grit-blasted
after roughening with an extra-fine diamond bur (Fig 5b). and ultrasonically cleaned groups, respectively. SEM im-
However, etching with phosphoric acid did not cause any ages and EDS analysis presenting the elemental mapping
morphological changes in the retentive pattern of the simi- of C, O, Si, and Al on the prepared composite surfaces are
larly treated composite, apart from producing a clean surface shown in Fig 6. Elemental compositions of the differently
(Fig 5c). Grit blasting with 50-μm Al2O3 particles produced a prepared surfaces are shown in Table 3.
rough, highly irregular surface topography, creating numerous
microretentive fissures (Fig 5d). Etching with phosphoric acid Surface Roughness Measurement
here also did not cause any morphological changes in the One-way ANOVA revealed a significant difference in surface
retentive pattern of the similarly treated composite surface, roughness between all surface treatment groups and the
apart from producing a cleaning effect (Fig 5e). Grit blasting control group. However, no significant difference was found
with 50-μm Al2O3 particles followed by ultrasonic cleaning among the surface treatment groups. Means and standard
produced similar surface texture to Fig 5d, but the surface deviations of surface roughness measurement are shown in
was less covered with Al2O3 particles (Fig 5f). Table 4.
EDS Analysis
From the SEM images of the prepared composite surfaces DISCUSSION
subjected to different surface treatments, remnants of alu-
minum abrasive particles were still observed on the grit- This study evaluated the effects of micromechanical and
blasted surface after phosphoric acid cleaning, and even chemical surface treatments on the repair bond strength of
after ultrasonication. The amount of aluminum was found to a resin composite. Surface treatment with grit blasting fol-
be 1.50 wt%, 0.25 wt%, and 0.16 wt% for the grit-blasted, lowed by silane application was selected as the recom-
Element (weight%)
Table 4 Mean surface roughness (Ra in μm) values and cantly higher than that of the control group. In addition, the
standard deviations according to different treatments macro- and microretentive features created by diamond bur
roughening could also lead to better surface wetting.4,9,34
Ra in μm The chemical bond also plays an important role in repair
Surface treatments (mean ± S.D.)
procedures.2,3,25,32 Silane treatment during repair proced-
Control 0.42 ± 0.06b ures promotes chemical bonding by forming siloxane bonds
Diamond bur 1.02 ± 0.06a between silica-containing filler particles exposed on the re-
Diamond bur with H3PO4 cleaning 0.97 ± 0.09a
pair surface and the resin matrix of the fresh resin
layer.12,17 According to the results of this study, the repair
Grit blasting with H3PO4 cleaning 1.05 ± 0.17a
bond strengths of the DSi and DPSi groups were higher than
Grit blasting with ultrasonic cleaning 1.08 ± 0.12a those of the D and DP groups, respectively (Fig 2). The sig-
Mean values with the same superscript letters are not statistically significantly nificant improvement of the repair bond strengths could be
different (one-way ANOVA and Duncan’s multiple comparison, p > 0.05). the result of the separate silane application.2,3,9,31,32 The
chemical effect of silane is also supported by the failure
analysis, as a lower incidence of adhesive failures was ob-
served in the groups in which silane was applied (Fig 3). In
addition, the benefit of a separate silane primer is in accor-
dance with Yoshihara et al,37 who demonstrated that the
mended protocol for composite repair.2,14 Surface rough- silane incorporated in Single Bond Universal adhesive was
ness was measured to evaluate the effect of mechanical not as effective as a separate silane primer in repair proced-
surface treatments, whereas EDS was performed for chem- ures. The incorporated silane was no longer stable, most
ical analysis. The long-term bond strength was evaluated likely because the low pH of Single Bond Universal pro-
after artificial aging with 10,000 cycles of thermocycling. motes hydrolysis and dehydration condensation of silanol.
According to the results of this study, surface treatment With phosphoric acid application, the repair bond
and the artificial aging demonstrated significant effects on strengths of the DP and DPSi groups were significantly
the repair bond strength of a resin composite using a uni- higher than those of the D and DSi groups, respectively.
versal adhesive (p ≤ 0.001). Therefore, both null hypothe- SEM images (Figs 5c and 5e) showed that the use of phos-
ses were rejected. phoric acid did not produce any significant micromorpho-
The repair bond strength of resin composite depends on logical changes in the retentive pattern of the composite
two main mechanisms: the micromechanical bond and the surface, and its action was limited to superficial clean-
chemical bond.7,11 The effect of the micromechanical bond ing.9,23 As a result, the surface roughness parameters were
is illustrated by the repair bond strengths of the D and DP similar (Table 4). Nevertheless, etching with phosphoric
groups, which were significantly higher than that of the con- acid might also promote the reactivity between a silica sur-
trol group. In our study, the resin composite blocks in the face and a silane coupling agent, and therefore increase
control group were only ground with 600-grit SiC paper in the number of Si–OH units on the silica surface.15
order to standardize the repaired surface. It has been re- Among the different repair protocols, the DPSi group
ported that the surface roughness created by diamond bur demonstrated the highest repair bond strength. Although
was significantly higher than that produced by SiC paper, the surface roughness values produced by diamond bur
resulting in increased surface area for bonding.26 This is in and grit blasting were similar, the repair bond strength of
agreement with surface roughness measurements the DPSi group was significantly higher than that of the
(Table 4), as the Ra of the D and DP groups were signifi- APSi group. The remnants of aluminum on specimens pre-
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